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08 BECK Art00baseclo Paillet P. (dir.) Les arts de la Préhistoire : micro-analyses, mises en contextes et conservation Actes du colloque « Micro-analyses et datations de l'art préhistorique dans son contexte archéologique », MADAPCA - Paris, 16-18 novembre 2011 PALEO, numéro spécial, 2014, p. 63 à 74 Programme ANR MADAPCA Chapitre 1 : ANALYSER 1b - Analyses non invasives Analyse non destructive des pigments préhistoriques : de la grotte au laboratoire Lucile BECK(1, 2), Matthieu LEBON(1, 3), Sophia LAHLIL(1, 3), Sylvain GRÉGOIRE(1), Giliane P. ODIN(1), Hélène ROUSSELIÈRE(1), Jacques CASTAING(1), Adrian DURAN(1), Colette VIGNAUD(1), Ina REICHE(1), Elsa LAMBERT(1), Hélène SALOMON(4, 5), Dominique GENTY(6), Laurent CHIOTTI(3), Roland NESPOULET(3), Frédéric PLASSARD(7), Michel MENU(1) Résumé : Les développements récents des méthodes d’analyse non destructives portables ou de laboratoire offrent de nouvelles possibilités pour l’étude de l’art préhistorique. Elles permettent maintenant de travailler sur les objets entiers, sans préparation ni prise de microéchantillon. Elles permettent aussi de réaliser des analyses dans les grottes et abris, directement sur les peintures et les dessins. Ces techniques donnent accès à un plus grand nombre de sites et d’objets d’intérêt puisqu’elles n’entraînent aucune destruction. Nous présentons dans cet article les développements analytiques les plus récents. Des investigations in situ ont été entreprises sur deux sites en Dordogne. Les études par fluorescence et diffraction X, spectrométrie Raman et réflectographie infrarouge dans les grottes de Villars et de Rouffignac ont permis de caractériser les pigments des dessins afin de mieux comprendre la réalisation des ensembles de figures et d’appréhender la gestion des matières premières. Certaines de ces techniques ont aussi offert la possibilité de dépister des éléments d’intérêt pour des applications spécifiques, comme par exemple la détection du carbone organique pour datation par radiocarbone. Au laboratoire, ce sont principalement la microdiffraction et l’émission X induite par particules chargées (PIXE) qui ont été employées pour l’étude des objets préhistoriques. Des études sur des objets colorés et blocs de pigments de deux sites ont été menées : la grotte du Renne à Arcy-sur-Cure (Yonne) et l’abri Pataud (Dordogne). Grâce à l’amélioration des limites de détection des éléments chimiques, il a été possible de différencier plusieurs sources pour la provenance des pigments ou encore de mettre en évidence des relations de composition chimique entre pigments bruts et objets décorés. Mots-clés : Fluorescence X, diffraction X, spectrométrie Raman, PIXE, pigments préhistoriques, grotte de Villars, grotte de Rouffignac, grotte du Renne à Arcy-sur-Cure. (1) C2RMF, UMR 171 CNRS, Centre de recherche et de restauration des musées de France, Palais du Louvre, Porte des Lions, 14, quai François Mitterrand, FR-75001 Paris - [email protected] (2) CEA, DEN, Service de recherches de métallurgie physique, Laboratoire Jannus, FR-91191 Gif-sur-Yvette (3) Muséum National d’Histoire Naturelle, département de Préhistoire, UMR 7194, 1 rue René Panhard, FR-75013 Paris (4) Centre européen d’archéométrie, Institut de Physique nucléaire, atomique et spectrométrie (IPNAS), Université de Liège, Sart Tilman- Bât. 15, B-4000 Liège (5) Univ. Bordeaux, UMR 5199, PACEA, Avenue des Facultés, FR-33405 Talence cedex (6) LSCE, UMR CEA/CNRS 8212, L’Orme des Merisiers, CEA Saclay, FR-91191 Gif-sur-Yvette cedex (7) SARL Grotte de Rouffignac, FR-24580 Rouffignac-Saint-Cernin 63 Les arts de la Préhistoire : micro-analyses, mises en contextes et conservation. Chapitre 1 : ANALYSER 1b : Analyses non invasives Abstract: Non-destructive analysis of prehistoric pigments, from the cave to the laboratory.The recent advances in non-destructive analytical methods with portable systems or in laboratory offer new possibilities to study Prehistoric art. First of all, it is possible now to work on whole objects, without preparation or micro-sampling. These non-destructive techniques also allow to carry out in situ analyses in caves and shelters on paintings and drawings directly. Consequently, they give access to a large number of sites and objects of interest. We present in this article the most recent analytical developments. In situ investigations were undertaken on two Prehistoric sites in Dordogne. In the caves of Villars and Rouffignac, we have characterized pigments by X-Ray fluorescence and diffraction, Raman spectrometry and infrared reflectography. These studies have contributed to a better understanding of the drawing panel organization and to the management of raw materials used as pigments. Some of these techniques have also offered the possibility of detecting elements of interest for specific applications as, for example, the detection of organic carbon for radiocarbon dating purpose. In the laboratory, micro-diffraction and Particle-Induced X-Ray Emission Spectrometry (PIXE) were mainly used for prehistoric objects. Studies on decorated objects and blocks of raw pigments from the Grotte du Renne in Arcy-sur-Cure (Yonne) and the Pataud Shelter in Les Eyzies (Dordogne) were investigated. Thanks to the improvement of the limits of detection of the chemical elements, it was possible to differentiate various sources for the pigment origin or to highlight chemical composition relationship between raw pigments and decorated objects. Key-words: X-Ray fluorescence (XRF), X-Ray diffraction (XRD), Raman spectrometry, PIXE, Prehistoric pigments, Villars cave, Rouffignac cave, Arcy-sur-Cure cave. Introduction - Analyses in situ : Les premières analyses chimiques des pigments ont Ces dernières années, des avancées importantes ont été commencé au début du XXe siècle, dès la découverte de réalisées dans la mise au point de systèmes portables. Ils l’art préhistorique (Moissan 1902). Dans les années 1990, utilisent différentes sources de rayonnements non destructifs (rayons X, infrarouges, laser de lumière visible). des études physico-chimiques ont été entreprises, livrant Grâce à ces systèmes d’analyse, il est maintenant possible des résultats significatifs sur la chaîne opératoire suivie par d’étudier un très grand nombre de peintures et de dessins les artistes du Paléolithique. On peut citer les travaux dans des abris ou des grottes. Les appareils développés ou portant sur les grottes ariégeoises, montrant diverses utilisés par le C2RMF pour les musées (fluorescence et préparations de pigment et de charge (Clottes et al. 1990 ; diffraction X, spectrométrie Raman et réflectographie IR), Menu et al. 1993), ou encore ceux consacrés à Lascaux où ainsi qu’un dispositif commercial de fluorescence X, ont été des analyses comparatives entre blocs de colorants et testés avec succès dans les grottes de Villars et de représentations pariétales sont présentées (Chalmin et al. Rouffignac. Ils ont été utilisés à plusieurs fins : 2004a ; Menu et Vignaud 2006 ; Vignaud et al. 2006). Par ailleurs, l’idée de « pots de peinture » pour l’élaboration des - caractérisation des pigments pour aider à la mains de la grotte de Gargas a été avancée (Menu et compréhension de la réalisation d’ensembles de figures et Walter 1992). La plupart de ces résultats ont été obtenus dessins et à l’appréhension de la gestion des matières sur de petits échantillons prélevés sur des peintures ou sur premières dans la grotte de Rouffignac ; des blocs de pigment facettés. Même si les prélèvements - dépistage d’éléments d’intérêt pour des applications sont de taille micrométrique, cette mise en œuvre limite le spécifiques, comme par exemple la détection du carbone nombre d’échantillons potentiels et s’avère impossible en pour datation par carbone 14 (voir Genty et al. 2014, ce cas d’objet unique ou particulièrement précieux. De plus, volume). les sources géologiques des pigments employés dans les cavités ont peu été identifiées, de telle sorte que la toute - Analyses au laboratoire : première étape de la chaîne opératoire, à savoir l’acquisition du pigment, est encore peu connue. Les rayons X sont utilisés depuis près d’un siècle pour l’étude des œuvres d’art en raison de leur innocuité à Les développements récents des méthodes d’analyse non l’échelle macroscopique (Beck 2011). Il existe différents destructives de laboratoire ou utilisant des appareils moyens de les mettre en pratique, qui conduisent à portables ont donné l’occasion d’entreprendre de nouvelles l’obtention d’informations complémentaires. C’est le cas approches pour l’étude de l’art préhistorique, en travaillant des deux méthodes utilisées au C2RMF pour la directement sur les objets ou en analysant in situ des caractérisation de pigments préhistoriques prélevés ou présents sur des objets qui peuvent être déplacés : peintures ou des dessins (Sanoit et al. 2005 ; Guineau et al. 2001). Dans le cadre de l’ANR Madapca, deux directions - la diffraction des rayons X (XRD pour X-Ray diffraction) de recherche sur des moyens d’analyse non destructifs des donne accès à la structure cristalline du (ou des) minéral pigments ont été menées : d’une part la mise en œuvre des (minéraux) formant le pigment. L’appareil de analyses in situ en grotte et d’autre part les microdiffraction (micro-XRD) récemment développé au développements effectués au laboratoire, au Centre de C2RMF permet la caractérisation des pigments sur objet recherche et de restauration des musées de France entier, évitant ainsi les prélèvements et la préparation (C2RMF). d’échantillons ; 64 Analyse non destructive des pigments préhistoriques : de la grotte au laboratoire - l’émission de rayons X, quant à elle, permet de connaître minéralogiques grâce à la diffraction de rayons X. la composition élémentaire du pigment, c’est-à-dire la L’appareil comprend une source (30 W, 40 keV et 700 µA) nature et la quantité des éléments chimiques présents. Elle de IFG (iMOX microfoyer) constituée d’un tube avec une peut être induite par divers types de rayonnements ; dans anode en cuivre (raie K-α du cuivre à E = 8,05 keV) isolé à le cas des faisceaux d’ions, il s’agit alors de la technique l’aide d’une fenêtre en béryllium de 0,01 mm et équipée de PIXE (Particle Induced X-Ray Emission).
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